基质分散固相萃取-气相色谱-质谱联用法测定塑料食品包装材料中9种光引发剂  

Determination of 9 photo- initiators residues in food plastic packaging by dispersive solid phase extraction coupled with gas chromatograph- mass spectrometry

作　　者：张居舟 尚光志 蔡荟梅[2,3] 陈贵杰[2,3] 彭传燚[2,3] 陶固帅 

机构地区：[1]安徽省食品药品检验研究院国家农副加工食品质量监督检验中心,安徽合肥230051 [2]安徽农业大学茶与食品科技学院,安徽合肥230036 [3]安徽农业大学省部共建茶树生物学与资源利用国家重点实验室,安徽合肥230036

出　　处：《食品工业科技》2015年第17期269-274,共6页Science and Technology of Food Industry

基　　金：国家现代农业(茶)产业技术体系(nycytx-26);国家质检总局科技计划项目-食品包装材料中紫外光引发剂迁移量的检测技术研究(2013zjjz007);安徽省自然科学基金项目(1408085MKL38);质检公益性行业科研专项项目(201310120)

摘　　要：建立了一种简单、快速检测食品塑料包装材料中9种光引发剂的分散固相萃取（d-SPE）净化、气相色谱-质谱联用（GC-MS）分析方法。样品用乙腈超声提取,提取液经氮吹,浓缩后,用150 mg无水Mg SO4、50 mg N-丙基乙二胺（PSA）和50 mg C18粉末分散固相萃取净化,用气相色谱/质谱（GC-MS）分析,采用选择离子监测（SIM）模式,外标法定量。9种光引发剂在0.02-1 mg/L范围内线性关系良好,线性相关系数（R2）均大于0.999。9种光引发剂在0.05,0.5和1 mg/L添加浓度下,回收率范围为82.9%-118.9%,相对标准偏差（RSD）为0.9%-10.5%,方法的定量限为0.07-0.33 mg/kg。该方法前处理简单,净化效果好,灵敏度和精密度均符合光引发剂检测的要求,适用于塑料食品包装材料中光引发剂残留的检测。A simple and rapid analytical method was established for the determination of 9 photo- initiators in the food plastic packaging by dispersive solid phase extraction（ d- SPE） coupled with gas chromatography- mass spectrometry（ GC- MS）. Photo- initiators were ultrasonically extracted by acetonitrile from samples,followed by concentrated under a stream nitrogen and then cleaned up by the mixed sorbents of 150 mg anhydrous Mg SO4,50 mg primary secondary amine（ PSA） and 50 mg octadecylsilane（ C18）. The ultimate solution was detected by GCMS with external standard method for quantitation under selected ion monitoring mode.All of the 9 photo- initiators had good linear relationships in the concentrations of 0.02 to 1 mg / L,and the R2 0.999.The recoveries of 9 photoinitiators were in the range of 82.9% -118.9% at three spike levels of 0.05,0.5 and 1mg / L,and the relative standard deviations（ RSD） were 0.9% -10.5%.The limit of quantification（ LOQ） for all analytes were range from 0.07 mg / kg to0.33 mg / kg.The method was sample,good purification effect,the sensitivity and precision meet the photo- initiator detection requirements,and it could be used for the determination of the residues of photo- initiators in the food plastic packaging.

关 键 词：光引发剂 分散固相萃取 塑料食品包装材料 气相色谱-质谱联用法 

分 类 号：TS206.4[轻工技术与工程—食品科学]